CN111044692A - Method for rapidly evaluating furfural substance content in liquid milk based on liquid milk heating temperature - Google Patents

Method for rapidly evaluating furfural substance content in liquid milk based on liquid milk heating temperature Download PDF

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CN111044692A
CN111044692A CN201911395019.XA CN201911395019A CN111044692A CN 111044692 A CN111044692 A CN 111044692A CN 201911395019 A CN201911395019 A CN 201911395019A CN 111044692 A CN111044692 A CN 111044692A
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邢倩倩
游春苹
刘振民
曹庆
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Bright Dairy and Food Co Ltd
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Abstract

The invention relates to the field of food, in particular to a method for rapidly evaluating the content of furfural substances in liquid milk based on the heating temperature of the liquid milk. The invention provides a method for rapidly evaluating the content of furfural substances in liquid milk based on the heating temperature of the liquid milk, which comprises the following steps: acquiring the heating temperature of the liquid milk; and evaluating the content of furfural substances in the liquid milk according to the heating temperature of the liquid milk, wherein the furfural substances are selected from hydroxymethyl furfural and furfural. The method for rapidly evaluating the content of the furfural substances in the liquid milk based on the heating temperature of the liquid milk can accurately and efficiently evaluate the content of the furfural compounds in the liquid milk only by the heating temperature of the liquid milk, is simple and rapid, has good accuracy, can be applied to monitoring the intake of dairy products and the like, and has good industrialization prospect.

Description

Method for rapidly evaluating furfural substance content in liquid milk based on liquid milk heating temperature
Technical Field
The invention relates to the field of food, in particular to a method for rapidly evaluating the content of furfural substances in liquid milk based on the heating temperature of the liquid milk.
Background
Dairy products have become an essential daily nutritional food as a recognized health drink. Cow's milk has long been an important part of people's daily diet in developed countries. The cow milk is rich in high-quality protein, fat, lactose, vitamins and calcium elements, has high utilization rate, and is a preferred source of natural calcium. In recent years, the government of China pays attention to the development of the dairy industry, greatly improves the milk yield and the consumption of residents, and puts the milk in an important position for improving the national health level. The raw milk and the products can be processed by different processes, mainly comprising pasteurization, ultra high temperature sterilization and the like.
The heat processing can effectively kill various pathogenic microorganisms in the raw milk, but can also affect the milk components. As the temperature of the heat treatment is increased, physical and chemical reactions such as denaturation and aggregation of whey protein, lactose isomerization and degradation, Maillard reaction and the like can occur in sequence, and the reduction of active ingredients (such as alkaline phosphatase, lactoferrin and the like) or the generation of reaction products (such as lactulose, furosine, furfural and the like) can be used as indicators of the hot processing strength. As one of representative products of the Maillard reaction, furfural compounds (mainly comprising hydroxymethyl furfural, furylmethyl ketone and methyl furfural) have functions of increasing aroma and adjusting color, but can cause harm to human bodies when reaching a certain dosage. The European food safety Committee recommends an upper limit of 1.6mg of hydroxymethylfurfural to be taken per person per day.
Therefore, monitoring of furfural compounds in dairy products is very important for the benign development of the dairy industry. In the prior art, the method for measuring the furfural compounds in the dairy products is relatively complex, so that a simpler and quicker method for measuring the furfural compounds in the dairy products is needed to be provided for monitoring the quality of the dairy products.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a method for rapidly estimating the content of furfural substances in liquid milk based on the heating temperature of the liquid milk, which is used for solving the problems in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a method for rapidly estimating the content of furfural in liquid milk based on the heating temperature of the liquid milk, which comprises:
(1) acquiring the heating temperature of the liquid milk;
(2) and evaluating the content of furfural substances in the liquid milk according to the heating temperature of the liquid milk, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
In some embodiments of the invention, the liquid milk is prepared from raw milk, preferably raw milk, after being subjected to a heat treatment.
In some embodiments of the invention, the heat treatment process of the liquid milk is selected from pasteurization, ultrapasteurization, or ultra high temperature sterilization.
In some embodiments of the present invention, the pasteurization may be performed at a temperature of 70 to 80 ℃ for 15 to 20 seconds.
In some embodiments of the present invention, the treatment temperature may be 120 to 138 ℃ and the treatment time may be 2 to 4 seconds in the ultra pasteurization.
In some embodiments of the invention, in the ultra-high temperature sterilization, the treatment temperature may be 135-140 ℃ and the treatment time may be 2-4 s.
In some embodiments of the present invention, the method for estimating the content of hydroxymethylfurfural in liquid milk according to the heating temperature of the liquid milk specifically comprises: and evaluating the content of the hydroxymethylfurfural in the liquid milk according to the heating temperature of the liquid milk by referring to a standard curve of the content of the hydroxymethylfurfural and the heating temperature of the liquid milk.
In some embodiments of the present invention, the equation of the standard curve of the content of hydroxymethylfurfural in the liquid milk and the heating temperature of the liquid milk is:
bx1
y1＝a·ebx1；
wherein x is1Representing the heating temperature of the liquid milk, and the unit is;
y1representing the content of hydroxymethylfurfuralUnit is mug/100 g;
a＝0.3402±0.5，b＝0.0378±0.05。
in some embodiments of the present invention, the method for estimating the furfural content in the liquid milk according to the heating temperature of the liquid milk specifically comprises: and evaluating the content of the furfural in the liquid milk according to the heating temperature of the liquid milk by referring to a standard curve of the content of the furfural and the heating temperature of the liquid milk.
In some embodiments of the present invention, the equation of the standard curve of the furfural content in the liquid milk and the heating temperature of the liquid milk is:
dx2
y2＝c·edx2；
wherein x is2Representing the heating temperature of the liquid milk, and the unit is;
y2represents the content of furfural with the unit of mu g/100 g;
c＝0.9017±1.0，d＝0.0084±0.005。
drawings
Fig. 1 is a graph schematically showing an equation fitted between hydroxymethylfurfural and heating temperature in example 1 of the present invention.
Fig. 2 is a schematic graph showing a fitting equation of furfural and heating temperature in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments, and other advantages and effects of the present invention will be apparent to those skilled in the art from the disclosure of the present specification.
After raw milk is subjected to heat treatment, as the temperature of the heat treatment increases, physicochemical reactions such as denaturation and aggregation of whey protein, isomerization and degradation of lactose, maillard reaction, and the like occur in sequence, and may result in reduction of active ingredients (e.g., alkaline phosphatase, lactoferrin, and the like), or production of reaction products (e.g., lactulose, furaldehyde, furfural, and the like). The inventor of the invention unexpectedly discovers through a large number of exploration experiments that the content of furfural compounds in liquid milk is related to the heat treatment process to which the liquid milk is subjected, particularly the content of hydroxymethylfurfural (CAS NO.67-47-0) and furfural (CAS NO.98-01-1) and the heat treatment temperature of the liquid milk have close relation, so that the content of furfural compounds in the liquid milk can be rapidly evaluated through the treatment temperature of the liquid milk, and the invention is completed on the basis.
The invention provides a method for rapidly evaluating the content of furfural substances in liquid milk based on the heating temperature of the liquid milk, which comprises the following steps:
(1) acquiring the heating temperature of the liquid milk;
(2) and evaluating the content of furfural substances in the liquid milk according to the heating temperature of the liquid milk, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
In the method for rapidly evaluating the furfural content in the liquid milk based on the heating temperature of the liquid milk, the liquid milk is generally prepared by raw milk after being subjected to heat treatment, the raw milk generally refers to normal milk which is directly extruded from the breasts of healthy milking animals, has no composition change, is not added with exogenous substances and has no processing, and can generally meet the relevant standards of TDTIA 001-2019, TDTIA 002-. The kind of liquid milk usually corresponds to the kind of raw milk. In a specific embodiment of the present invention, the raw milk may be raw milk or the like, and the liquid milk may be milk or the like.
In the method for rapidly evaluating the content of the furfural substances in the liquid milk based on the heating temperature of the liquid milk, the heating temperature of the liquid milk generally corresponds to the heating temperature in the heat treatment process of the raw milk in the preparation process of the liquid milk. In the present invention, the heat treatment to which the raw milk is subjected during its preparation is generally unitary, i.e. it is subjected to a heat treatment in which the heating temperature used is only within a certain temperature range, which typically does not fluctuate more than 3 ℃.
In the method for rapidly evaluating the content of the furfural substances in the liquid milk based on the heating temperature of the liquid milk, the heating temperature of the liquid milk usually depends on the heat treatment process of the liquid milk. Generally, the heat treatment process to which the raw milk is subjected depends mainly on the treatment temperature (i.e., heating temperature) and the treatment time (i.e., heating time) of the process, with higher heating temperatures generally combined with shorter treatment times and lower heating temperatures generally combined with longer treatment times, thereby achieving good sterilization effects. In an embodiment of the present invention, the treatment time may be 15 to 20 seconds at a heating temperature of 70 to 95 ℃, and the treatment time may be 2 to 4 seconds at a heating temperature of 120 to 140 ℃. Suitable heat treatment processes for raw milk will be known to the person skilled in the art, and may in particular be pasteurisation, ultra-pasteurisation, or ultra-high temperature sterilisation, for example. In an embodiment of the present invention, in the pasteurization, the treatment temperature may be 70 to 80 ℃ and the treatment time may be 15 to 20 seconds. In another embodiment of the present invention, the treatment temperature in the ultra pasteurization can be 120 to 138 ℃, and the treatment time can be 2 to 4 seconds. In another embodiment of the present invention, in the ultra-high temperature sterilization, the treatment temperature may be 135 to 140 ℃ and the treatment time may be several seconds, for example, 2 to 4 seconds.
According to the method for rapidly evaluating the content of furfural substances in the liquid milk based on the heating temperature of the liquid milk, provided by the invention, the content of hydroxymethylfurfural in the liquid milk can be evaluated according to the heating temperature of the liquid milk. The evaluating the content of the hydroxymethylfurfural in the liquid milk according to the heating temperature of the liquid milk may specifically include: and evaluating the content of the hydroxymethylfurfural in the liquid milk according to the heating temperature of the liquid milk by referring to a standard curve of the content of the hydroxymethylfurfural and the heating temperature of the liquid milk. As mentioned above, there is a close relationship between the content of hydroxymethylfurfural in the liquid milk and the heat treatment temperature of the liquid milk, and generally speaking, the higher the content of hydroxymethylfurfural, the higher the heat treatment temperature of the liquid milk. And evaluating the content of the hydroxymethylfurfural in the liquid milk according to the heating temperature of the liquid milk by a pre-established standard curve of the content of the hydroxymethylfurfural and the heating temperature of the liquid milk. In an embodiment of the present invention, the equation of the standard curve of the content of hydroxymethylfurfural in the liquid milk and the heating temperature of the liquid milk is as follows:
y1＝a·ebx1；
wherein x is1Representing the heating temperature of the liquid milk, and the unit is;
y1represents the content of the hydroxymethylfurfural with the unit of mu g/100 g;
the value of a can be 0.3402 + -0.5, 0.3402 + -0.4, 0.3402 + -0.3, 0.3402 + -0.2, 0.3402 + -0.1, 0.3402 + -0.05, 0.3402 + -0.03, 0.3402 + -0.01, 0.3402 + -0.005, 0.3402 + -0.003 or 0.3402 + -0.001; the value of b can be 0.0378 + -0.05, 0.0378 + -0.04, 0.0378 + -0.03, 0.0378 + -0.02, 0.0378 + -0.01, 0.0378 + -0.005, 0.0378 + -0.003, 0.0378 + -0.001, 0.0378 + -0.0005, 0.0378 + -0.0003 or 0.0378 + -0.0001.
According to the method for rapidly evaluating the content of the furfural substances in the liquid milk based on the heating temperature of the liquid milk, provided by the invention, the content of the furfural substances in the liquid milk can be evaluated according to the heating temperature of the liquid milk. The estimating of the furfural content in the liquid milk according to the heating temperature of the liquid milk may specifically include: and evaluating the content of the furfural in the liquid milk according to the heating temperature of the liquid milk by referring to a standard curve of the content of the furfural and the heating temperature of the liquid milk. As mentioned above, there is a close relationship between the furfural content in the liquid milk and the heat treatment temperature of the liquid milk, and generally speaking, the higher the furfural content, the higher the heat treatment temperature of the liquid milk. And evaluating the content of the furfural in the liquid milk according to the heating temperature of the liquid milk by a pre-established standard curve of the content of the furfural and the heating temperature of the liquid milk. In an embodiment of the present invention, the equation of the standard curve of the furfural content in the liquid milk and the heating temperature of the liquid milk is:
y2＝c·edx2；
wherein x is2Representing the heating temperature of the liquid milk, and the unit is;
y2represents the content of furfural with the unit of mu g/100 g;
the value of c can be 0.9017 + -1.0, 0.9017 + -0.8, 0.9017 + -0.6, 0.9017 + -0.4, 0.9017 + -0.2, 0.9017 + -0.1, 0.9017 + -0.05, 0.9017 + -0.03 or 0.9017 + -0.01; the value of d can be 0.0084 + -0.005, 0.0084 + -0.004, 0.0084 + -0.003, 0.0084 + -0.002, 0.0084 + -0.001, 0.0084 + -0.0005, 0.0084 + -0.0003 or 0.0084 + -0.0001.
The evaluation method of the heat treatment process of the liquid milk provided by the invention can accurately and efficiently evaluate the content of furfural compounds (such as hydroxymethyl furfural, furfural and the like) in the liquid milk only by the heating temperature of the liquid milk, has the advantages of simple and rapid method, good accuracy, application to monitoring the intake of dairy products and the like, and good industrialization prospect.
The invention of the present application is further illustrated by the following examples, which are not intended to limit the scope of the present application.
Example 1
Establishing a fitting equation of the heating temperature of the liquid milk, the content of the hydroxymethyl furfural and the content of the furfural:
the heat treatment is carried out on the raw milk by simulating different heating conditions, wherein the heat treatment is respectively carried out at 70 ℃/15s, 75 ℃/15s, 80 ℃/15s, 85 ℃/15s, 90 ℃/15s, 95 ℃/15s, 120 ℃/4s, 125 ℃/4s, 130 ℃/4s, 135 ℃/4s, 137 ℃/4s, 139 ℃/4s and 140 ℃/4s (before "/" is the temperature of heat treatment, after "/" is the time of heat treatment), the fat content of the used raw milk (taken from a certain pasture in Shanghai) is 4.15 percent, the lactose content is 5.42 percent, the protein content is 3.39 percent, and the solid content of the non-fat milk is 9.05 percent.
The method for detecting the content of the furfural compounds in the liquid milk after different thermal processing comprises the following steps:
(1) weighing 15g of liquid milk sample, adding 4.5ml of 0.16mol/L of oxalic acid prepared on the same day, heating in a water bath at 90 ℃ for 30min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 35g/mL, shaking for 10min, and centrifuging for 18min at 4 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 3.5g/mL trichloroacetic acid solution B into the filter residue, shaking for 10min, and centrifuging for 18min at 4 g; the supernatant is combined, and 3.5g/mL trichloroacetic acid solution B is added to the volume to be calibrated.
(3) Taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 2.7 mu m, wherein the chromatographic column comprises the following components in percentage by weight: WatersatlantIST3(2.8 mm. times.12 cm, 2.8 μm); mobile phase: the mobile phase A is water, and the mobile phase B is acetonitrile; gradient elution: 0-10.0min, 5% B-95% B, 10.0-12.0min, 95% B-95% B, 12.0-12.1min, 95% B-5% B, 12.1-20.0min, 5% B-5% B; the flow rate is 0.5 mL/min; temperature of the column: 28 ℃; sample introduction amount: 4.5 mu L; temperature of a sample injection tray: 3.8 ℃; ultraviolet detection wavelength: 270 nm.
The results of the analysis of the liquid milk obtained in each thermal treatment are shown in table 1:
TABLE 1
Figure BDA0002346065320000061
Based on the content of the hydroxymethylfurfural under different heating conditions, establishing a fitting equation of the heating temperature and the content of the hydroxymethylfurfural:
y1＝0.3402e0.0378x1(i)；
wherein x is1Represents the heating temperature of the liquid milk, and the unit is;
y1representing the content of the hydroxymethylfurfural in the liquid milk, and the unit is mu g/100 g;
the curve of the fitted equation is shown in figure 1.
Based on the furfural content under different heating conditions, establishing a fitting equation of the heating temperature and the furfural content:
y2＝0.9017e0.0084x2
wherein x is2Represents the heating temperature of the liquid milk, and the unit is;
y2represents the furfural content in the liquid milk, and the unit is mug/100 g.
The curve of the fitted equation is shown in fig. 2.
Example 2
Verification of the accuracy of the fitting equation:
sample A, B, C, D is a laboratory process simulation product (non-commercial sample), and the specific information for each sample is as follows:
sample a: is obtained by processing raw milk, and the specific parameters of the raw milk are as follows: the fat content is 4.15%, the lactose content is 5.42%, the protein content is 3.39%, the non-fat milk solid content is 9.05%, the heat treatment conditions are 75 ℃, 85 ℃ and 95 ℃ respectively, and the treatment time is 15 s;
sample B: is obtained by processing raw milk, and the specific parameters of the raw milk are as follows: 5.15% of fat, 5.52% of lactose, 3.93% of protein and 9.85% of non-fat milk solid, wherein the heat treatment conditions are 130 ℃, 135 ℃ and 137 ℃, and the treatment time is 4 s;
sample C: is obtained by processing raw milk, and the specific parameters of the raw milk are as follows: the fat content is 4.17 percent, the lactose content is 5.96 percent, the protein content is 3.40 percent, the non-fat milk solid content is 9.03 percent, the heat treatment conditions are respectively 75 ℃, 85 ℃ and 95 ℃, and the treatment time is 15 s;
sample D: is obtained by processing raw milk, and the specific parameters of the raw milk are as follows: fat content 4.13%, lactose content 4.90%, protein content 3.49%, non-fat milk solid content 9.06%, heat treatment conditions of 130 deg.C, 135 deg.C and 137 deg.C, and treatment time of 4 s;
according to the heating temperatures of A, B, C and D, the theoretical content of furfural substances in the sample is calculated by the standard curve given in example 1, and the actual content of hydroxymethylfurfural and furfural is further detected by the detection method for the content of furfural compounds in liquid milk provided in example 1, and the specific results are shown in Table 2:
TABLE 2
Figure BDA0002346065320000071
As can be seen from the related results in Table 2, the evaluation result of the heating temperature obtained by furfural substances has a high degree of conformity with the actual heating temperature, which indicates that the heating temperature of the liquid milk can be accurately detected by the above method.
In conclusion, the present invention effectively overcomes various disadvantages of the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. A method for rapidly evaluating the content of furfural substances in liquid milk based on the heating temperature of the liquid milk comprises the following steps:
(1) acquiring the heating temperature of the liquid milk;
(2) and evaluating the content of furfural substances in the liquid milk according to the heating temperature of the liquid milk, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
2. The method for evaluating the heat treatment process of liquid milk according to claim 1, wherein the liquid milk is prepared from raw milk, preferably raw cow's milk, after being subjected to a heat treatment.
3. The method for evaluating the heat treatment process of liquid milk according to claim 1, wherein the heat treatment process of liquid milk is selected from the group consisting of pasteurization, ultrapasteurization, and ultra high temperature sterilization.
4. The method for evaluating the heat treatment process of liquid milk according to claim 3, wherein the pasteurization is carried out at a temperature of 70-80 ℃ for 15-20 s.
5. The method for evaluating the heat treatment process of liquid milk according to claim 3, wherein the ultra pasteurization is performed at a temperature of 120 to 138 ℃ for 2 to 4 seconds.
6. The method for evaluating the heat treatment process of the liquid milk according to claim 3, wherein in the ultra-high temperature sterilization, the treatment temperature can be 135-140 ℃ and the treatment time can be 2-4 s.
7. The method for evaluating the heat treatment process of the liquid milk according to claim 1, wherein the method for evaluating the content of the hydroxymethylfurfural in the liquid milk according to the heating temperature of the liquid milk specifically comprises the following steps: and evaluating the content of the hydroxymethylfurfural in the liquid milk according to the heating temperature of the liquid milk by referring to a standard curve of the content of the hydroxymethylfurfural and the heating temperature of the liquid milk.
8. The method for evaluating the heat treatment process of liquid milk according to claim 1, wherein the equation of the standard curve of the content of hydroxymethylfurfural in the liquid milk to the heating temperature of the liquid milk is as follows:
y1＝a·ebx1；
wherein x is1Representing the heating temperature of the liquid milk, and the unit is;
y1represents the content of the hydroxymethylfurfural with the unit of mu g/100 g;
a＝0.3402±0.5，b＝0.0378±0.05。
9. the method for evaluating the heat treatment process of the liquid milk according to claim 1, wherein the method for evaluating the furfural content in the liquid milk according to the heating temperature of the liquid milk specifically comprises: and evaluating the content of the furfural in the liquid milk according to the heating temperature of the liquid milk by referring to a standard curve of the content of the furfural and the heating temperature of the liquid milk.
10. The method for evaluating a heat treatment process of liquid milk according to claim 9, wherein the equation of the standard curve of the furfural content in the liquid milk and the heating temperature of the liquid milk is as follows:
y2＝c·edx2；
wherein x is2Representing the heating temperature of the liquid milk, and the unit is;
y2represents the content of furfural with the unit of mu g/100 g;
c＝0.9017±1.0，d＝0.0084±0.005。
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Publication number Priority date Publication date Assignee Title
CN111596015A (en) * 2020-05-28 2020-08-28 光明乳业股份有限公司 Method for evaluating liquid milk heating process based on furfural substance content in liquid milk
CN111739590A (en) * 2020-07-01 2020-10-02 光明乳业股份有限公司 Method for predicting content of hydroxymethylfurfural and furfural in normal-temperature yogurt based on storage temperature and storage time
CN111739590B (en) * 2020-07-01 2022-10-04 光明乳业股份有限公司 Method for predicting content of hydroxymethylfurfural and furfural in normal-temperature yogurt based on storage temperature and storage time
CN111983158A (en) * 2020-08-20 2020-11-24 光明乳业股份有限公司 Method for rapidly identifying doping amount of reconstituted milk in raw milk
CN112986437A (en) * 2020-12-30 2021-06-18 光明乳业股份有限公司 Purification detection method for furfural compounds in coffee dairy products
CN115316438A (en) * 2021-05-10 2022-11-11 中粮营养健康研究院有限公司 Dairy simulation system and application thereof, edible dairy and preparation method thereof

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